Process of forming methyl alcohol and other compounds from waste liquors containing organic matter.



A. H. WHITE. PROCESS OF FORMING METHYL ALCOHOL AND OTHER COMPOUNDS FROM WASTE LIQUORS CONTAINING ORGANIC MATTER.

APPLICATION FILED NOV- 29, I915- I yfififio Patented Sept 12, 1916.

barren s'rATies rairnu'r oimiiou.

ALFRED H. WHITE, ANN ARBOR, MICHIGAN.

rnocnss or FORMING METHYL ALCOHOL AND 'oTrrEn COMPOUNDS rrwivr WASTE LIQUORS CONTAINING ORGANIC MATTER.

To all whom it may concern: 1 r

Be it known that I, ALFRE H. WHITE, a

citizen of the United States of .America,

residing at Ann Arbor, in the county of.

' Liquors Containing Organic Matter," of

which the following is a 'specificatiom; reference being had therein to the accompany mg drawings. I

The invention relates to improvements in if i the methods of destructive distillation of liquids containing large amounts of organic matters in solution or suspension and 1H particular to the recovery of f methyl' alcohol,

acetone and other Valuableproducts destructive distillation. I

n is well known that in rocesse or as: structive distillation theremu-st be'regulation not only of temperature and pressure but also of time and contact "surfacel In the destructive v distillation of 'organic'-' sub-v. stances containing large amounts of"oxygen such as wood there is an fexothermicreac g tion at one stageof the processwhichfinfthe usual practice causes a material rise in tem perature and disturbs the smooth course of. the reaction. I have discovered'that when such substances are inthe form of liquids so that it is possible to introdu'cethem "into! the retort continuouslyor in Small portions,

it is possible not only to control but to take advantage of this exothermic reaction to maintain uniform conditions of destructive distillation, and I have been able .towork out advantageous processes for the utilize-i tion of what have hitherto been waste prod- E is adi-vision wall for compelling the prod- 'uctsf'of combustion ascending from the grates to descend adjacent the opposite ends of the retorts to the escape flue F. This note.

manufacturing wood pulp by the'soda process, but is applicable-to other liquids carry ing large amounts of organic matters in solu:

tion or suspension. In the usual processthese 1 liquors are concentrated to a thick, syrup and then burned for the recovery of soda, but with the entire loss of the organicmatters. It has been hitherto impracticable to subject these to destructive distillation because of their tendency to foam and because of the exothermic reaction occurring at one The process here described is for -the.- utilization of the wasteliquors fromjmills.

Specification of Letters Patent. I Patentqgd Sept- 12, 191083,, Application filed November 29, 1915. SeriaiNo. 64,156.

1 stage of theprocess. These difficulties are obviated in my process and an exact control of conditions is allowed.

I have discovered that the quantities of methyl alcohol and acetone obtained from the destructive distillation. of this liquor vary markedly Withthe conditions and have determined what the conditions must. be to secure advantageous yields. For commercial reasons the operations are carr ed out at almostnormal atmospheric'pressure, but the temper ature,time of heating and extent of contact substance are controlled. A variation in any oneof these factors affects the others, and in general the higher the v temperature within certain limits and the greater the amount of contacting surface the shorter the time required for treatment.

Also I have found that the temperature of the Vapor space-should not be less than 450 F. or inorethan 750 F. and that the time oft-reatment .of the vapors within the re tortfsh'ould bewithin the limits of to 150 seconds; i .In the drawings I have illustratedone specific form of apparatus adapted for the carrying out of my process, Figure 1 illusitrating. a longitudinal section and Fig. 2

an end elevation.

extending through the opposite walls of the furnace. These retorts are'also preferably provided withqremovable caps C to facilitateljthe cleaningof the same and removal =of -carbon depos'its.' As shown D is the grate arranged beneath one end of the retorts ain't by suitable means, such as the trap feed conduit G which preferably extends into the ere the 5 it, not so .essentiz 'liquo adm'nta ecus; te f the retort is relatively I ng-he temperatures, ,l1owe\fer,

drawn =ofi thiio'ugli p witlrt-he-several retorts. Theblack ash acts I as a catalyzer 'eand in -t is ape-city; is' of metastasis at .ra porg within the vretort$1,

, pr c'ef'ss is 'that1thefseyeral rare;

he' p'r cesss. v

ffiow b the quid-is j reg ulated rei ipie tli r c haying obtain d; by. such itreatmen a ilistillate -,con%

taming; a muchras 4.9 ip'ericent f. volume alcohola ndacetone Y The-time durin'g' wlri in the reto'rt'lmuslt depend iiipior'i' t-h liquid is admitted the "faster it will ya temperatur must be correspondinglychan d withi one ot' headvantageous features of n at-are; rate i flow and amoun may be, separately controlled; thus the best. results according,-

' 4 tortiseventuallytilled or largely;:fillerlwith the black ash and as frequently as necessary this may io'eremoved bycpeninL the s C at the opposite endsdffthe eto'rti iid' fforc'ingft I merit.

, .i l ii v x y N that. aritlrmy, process thegliquid duced directly into. ether heated; Z 11 destructive distillation takes-place; anditliat in this heated chamberitisspread out over an extended contact surfacci- This contact the -var product is -\COIld1 1llil J connected degrees oldin g the chthe "Vapors are retained: with- 0f; admission offfthe' ,liquidj' sinicethe ast'r'ithe 'rizef h e e the pre ie at aiallb fg a .more rapidly itymust be displaced; Und .Yaried conditions of; 35,--

er; and amount of contact surfa ce: the crate 0- new I he .I am enabled to vary conditions asljto l obtain ie il t'ewh used and the products desrred .;J I.-his-.also

layer and: "is rapidly 'subJectGd to destructive distillatioii a-ndmaintainmg. the temperav ture w thin the yaporspacc from 550 to 600 (call t. the

or a local high temperature of the black ash.

The liquid flowing over this contact surface is of. a much lower temperature, which prevents carbonization within'the body of the liquid and thus avoids the formation of a I sticky mass diflicultto manipulate. In other wordsgvithmy process I obtain without the useofmechamcal agltators a constant feedingof the material into the retort and uniform treatment of the material thus fed in throughout the entire process. This together with the accurate control of tempcra- -ti 1res,rate of flow and amount of contact surface enables me to obtain a higher yield ofthedesired product than has heretofore been possible.

I Asia result of the introduction of the liquorfdirectlyinto the heated .zone of the retortevaporation and destructive distillation are carried on simultaneously so that the'gaseous products of the destructive distillation are commingled with the water vano wi'thin-the retort,.which is a condition fti't orable tola higlr yield of the desired ec -q 4 hebuilding up of the black ash upon fnerjsurface of the retort it is evident rb'oni'zation willta' ke place more raphere the -.surf-ace is hottest. This tends to equalize,Ytemperature conditions within theret'ort gforthe, porous coatingacts as 'a' heat insulatoraiid therefore the increased deposit; on the hot surface will diminish the I of heat conduction; ,7 i j .cla'im asfn yfinvention is The process f'ofform'ing yaluable prodacts from waste liquors; containing organic matter eomprising the; gradual introduci 1 tive distillation, and. maintaining the vapor v p p I x within sai'dretort at a temperature from 450 .-In I the continuation of thesprocess h the liquor. intoa' retort for destruc- 'lfio s'econdsqT- y 2. ,Theprocessof manufacturing methyl alcohol, acetone and other ialuable products fuf'asteg li'quors. of .mills manufacturing ot 11111 1 3 the soda process, comprising e;tliei concentrated liquor gradually a retort, where it spreads out in a thin degrees F.

8. The process of manufacturing methyl memes alcohol, acetone and other valuable products from waste liquors of millsla'nanufacturing wood pulp by the soda process, comprising feeding the concentrated liquor gradually into a retort maintained ata temperature between 150 and 700. degrees F., in which retort the liquor is spread out in a thin layer and is rapidly subjected to destructive distillation, and regulating-the rate of feed tomaintain' the gases within the retort from 5 to 150 seconds varying with the temperature and the amount of contact surface which acts as a catalyzer. I, 1

I 4. The process of manufacturing methyl alcohol, acetone and other valuableproducts from waste .liquors of mills manufacturing Woodpulp by the soda process, comprising feeding the concentrated liquor gradually.

into a retort heated from 450 to 700 degrees F., where it spreads out in a thin layerand is rapidly subjected to destructive distillar 'tion' attended with foaming and charring' which fills the space with a porous black ash, andregulating the rate of feed to maintain the: vapor in the retort from 5 to 150 seconds varying according to the; temperature and amount of'contact substance actlng as a catalyzer, the time being increased for low temperatures and decreased for higher temperatures. i

5. The process 'of manufacturing methyl alcohol, acetone and othervaluable products from the aste liquors of millsmanufactun ing wood pulp by the soda process, comprising feeding the concentrated liquor gradually into a heated retort, andregul'ating the rateof flow. and the external heating of the J retort to control theexothermic reaction and to maintain the vapors Within the. retort under a temperaturefrom 450 to 700 degrees F. and for a time varying from 5 to 150 seconds a I v 6. The process of forming valuable products from waste liquors containing organic matter, comprising feeding the concentrated I liquor gradually directly into a zone of a tort having a temperature above that of destructive distillation, and spreading the liquor into a comparatively thin layer before it] attains the temperature of destructive distillation. I

8. The process of manufacturing valuable products from waste liquors containing organic matter, comprising the feeding of con centrated liquor having a temperature'less than {that of destructive distillation directly into a retortheat'ed to above the point of destructive,distillation and'in contact with by vaporization ofthe water iscarried on porous charcoal acting as a catalyzer, Wheresimultaneously with destructive distillation and affects the reaction.

9.7 The process of securing destructlve dis- 7 tillation of liquors containing organic matter'at constant temperature, comprising the flowing of the liquid over a heated surface to form a carbonaceous deposit thereon, said deposit being of greater thickness where the surface is hottest, and thereby forming a heat insulator which equalizes the temperature of all portionsof the contact surface '10; In a process of securing destructive distillation of liquid containing organic matter, the step of flowing thin layers of the liquid into a retort over a freshly formed carbonaceous contact surface, through which where the destructive distillation continues. 7

the heat for destructivedistillation istransmitted to the liquor. I

11. The process of securing destructive distillation of thinlayers of liquidcontaining organic matter, comprising'the flowing of the liquor into a retortover a freshly formed carbonaceous contact surface through which the heat for destructive distillation is transmitted to the liquor, and protecting the liquid in contact with said surface from,

radiant heat by thesuperposed layer of undistilled liquid flowing there'over.

' -12. The process of -securing destructive 1 distillation v of thin layers of liquid containing organic matter, comprising flowing the liquor into a retort over aheated surface to form a carbonaceous deposit thereon, automatically increasing in thickness at the points where the metal is hottest and there by equalizing the temperature of the carbo- .naceous contact with the liquid and protecting the liquidin contact with said surface from radiant heat by the superposed layer of liquid fiowingthereover. v

' In testimony whereof I aiiix my signature in presence of two witnesses ALE-RED H.'WTHITE.

I -Witnesses:

' JAMES P. BARRY, PHYLLIS CoBURN. 

